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Preparation method of prop-1-ene-1, 3-sultone

A technology of sultone and propylene, which is applied in the field of preparation of organic materials, can solve the problems of low yield of cyclosynthesis products and slow reaction speed, and achieve the effects of high yield, fast reaction speed and reduced production cost

Active Publication Date: 2015-04-29
SHIJIAZHUANG SAN TAI CHEM CO LTD
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Problems solved by technology

[0004] The present invention proposes a preparation method of 1-propene-1,3-sultone, which is used to solve the problems of slow reaction speed in the cyclosynthesis reaction step and low yield of cyclosynthesis products in the existing preparation method

Method used

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  • Preparation method of prop-1-ene-1, 3-sultone

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preparation example Construction

[0030] Such as figure 1 Shown: a kind of preparation method of 1-propene-1,3-sultone, comprising the following steps:

[0031] The first step, add:

[0032] The reaction raw material propargyl alcohol and the reaction raw material alkali metal sulfite or bisulfite carry out addition reaction in aqueous solution;

[0033] The second step, acidification:

[0034] After the addition reaction is finished, add acid to stop the reaction, the amount of acid added makes the pH value of the reaction solution reach below 4, filter to obtain the acidified filtrate;

[0035] The third step, esterification ring synthesis:

[0036] Heating the acidified filtrate to carry out the cyclosynthesis reaction, the temperature of the cyclosynthesis reaction is 100-180°C, the reaction time is 1-2 hours, the cyclosynthesis reaction is carried out under the pressure of 1-10mmHg and catalyst catalysis, until no liquid is evaporated.

[0037] The reaction equation for the addition reaction is:

[0...

Embodiment 1

[0060] Example 1: Select 200 g of the filtrate after salt extrusion (i.e. after acidification) prepared as above, the catalyst is 5 g of hydrochloric acid gas, and cyclize under a vacuum of 10 mmHg for 1 to 2 hours, and separate according to the separation technology in the comparative example, and finally obtain PST crude product 133g, yield is 77.7%.

[0061] The above catalyst hydrochloric acid can be replaced by an equivalent amount of sulfuric acid, phosphoric acid, nitric acid or gaseous mineral acid.

Embodiment 2

[0062] Example 2: Select 200 g of the filtrate after salt extrusion (i.e. after acidification) prepared as above, the catalyst is 5 g of hydrochloric acid gas, and ring-close for 1 to 2 hours under a vacuum of 1 mmHg, and separate according to the separation technology in the comparative example, and finally obtain PST crude product 139g, yield is 81.2%.

[0063] The above catalyst hydrochloric acid can be replaced by an equivalent amount of sulfuric acid, phosphoric acid, nitric acid or gaseous mineral acid.

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Abstract

The invention provides a preparation method of prop-1-ene-1, 3-sultone in order to solve the problems of low reaction speed in a cyclo-synthesis reaction step and low product yield in the existing preparation method. The preparation method comprises the following operation steps of firstly, carrying out addition reaction, namely carrying out addition reaction on reaction raw materials, namely propynol and alkali metal sulfite or bisulfite, in a water solution; secondly, acidifying, namely adding acid to stop the reaction after the addition reaction is ended, and filtering to obtain acidified filtrate, wherein the addition quantity of the acid is controlled according to the requirement that the pH value of the reaction solution is less than 4; and thirdly, carrying out esterification and cyclo-synthesis, namely heating the acidified filtrate to carry out cyclo-synthesis reaction at the temperature of 100-180 DEG C and the pressure of 1-10mmHg for 1-2 hours under the action of a catalyst until no liquid is evaporated. The preparation method of prop-1-ene-1, 3-sultone, provided by the invention, has the advantages of simplicity in operation, high cyclo-synthesis reaction speed, high product yield as well as low wastewater, water gas and waste residue yield, so that the preparation method can be used for industrial application and popularization.

Description

technical field [0001] The invention relates to the technical field of preparation of organic materials, in particular to a preparation method of 1-propene-1,3-sultone. Background technique [0002] 1-propene-1,3-sultone (referred to as PST) is an important pharmaceutical intermediate. Its unique structure makes it irreplaceable in the synthesis of heterocyclic drugs. It can also be used as lithium Additives for battery electrolyte, used to prolong the service life of lithium batteries. [0003] Patent 200910073620.7 (publication number 101456856, publication date June 17, 2009) proposes a method for the preparation of 1-propene-1,3-sultone, using addition, acidification, and cyclosynthesis processes to prepare PST products. The specific technical scheme of the cyclization reaction is: heating the cyclization, the cyclization temperature is 100-180° C., and the cyclization is carried out under normal pressure or reduced pressure until no liquid is evaporated. In the embodi...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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